CN112501909B - 一种抑菌纤维膜材料及其制备方法及抑菌纤维膜口罩 - Google Patents
一种抑菌纤维膜材料及其制备方法及抑菌纤维膜口罩 Download PDFInfo
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Abstract
本发明公开了一种抑菌纤维膜材料及其制备方法及抑菌纤维膜口罩,抑菌纤维膜材料的制备方法包括以下步骤:S1:制备聚氨酯/木质素纤维膜;S2:向制得的聚氨酯/木质素纤维膜中加入杜仲提取物溶液,加热,调节pH反应后,得到抑菌性能的纤维膜材料。采用本发明提供的方法制备的纤维膜更加环保、具备可降解性,并且将杜仲提取物应用在口罩材料上,提高口罩的抑菌性能,因此本发明提供的纤维膜材料是一种安全无毒、具有高效抑菌性能的纤维膜材料。
Description
技术领域
本发明属于口罩材料技术领域,尤其涉及一种抑菌纤维膜材料及其制备方法及抑菌纤维膜口罩。
背景技术
作为阻挡外界细菌和病毒进入人体呼吸道的防护产品,口罩材料的选择越来越受到人们的重视。但口罩材料的性能特点使得其本身也是细菌附着繁殖的良好介质。抑菌性能的引入对于口罩的发展具有重要意义。因与人体直接接触,抗菌剂需满足安全无毒的要求,钙与杜仲提取物中的绿原酸形成的螯合物具有良好的抗菌性能和生物相容性,是理想的抗菌剂选择,但是常规制备方法对制备设备要求高,耗能大,或会对环境带来破坏。
发明内容
本发明提供了一种抑菌纤维膜材料及其制备方法及抑菌纤维膜口罩,采用本发明提供的方法制备的纤维膜更加环保、具备可降解性,并且将杜仲提取物应用在口罩材料上,提高口罩的抑菌性能,因此本发明提供的纤维膜口罩材料是一种安全无毒、具有高效抑菌性能的纤维膜口罩材料。
为实现上述目的,本发明的技术方案为:
一种抑菌纤维膜材料的制备方法,包括以下步骤:
S1:制备聚氨酯纤维膜;
S2:向制得的聚氨酯纤维膜中加入杜仲提取物溶液,加热,调节pH反应后,得到抑菌性能的纤维膜材料。
为了使抑菌效果更持久,优选地,在所述步骤S2中:首先将制得的聚氨酯纤维膜置于氯化钙溶液中,加热后再加入杜仲提取物溶液,调节pH反应后,得到抑菌性能的纤维膜材料,将氯化钙与杜仲提取物中的绿原酸反应,获得螯合物,使抑菌性能更持久。
优选地,所述聚氨酯纤维膜的具体制备方法为:配置热塑性聚氨酯溶液,将氯化锂和碱木质素加入到配置的热塑性聚氨酯溶液中,搅拌、溶解;然后通过静电纺丝设备制备聚氨酯/木质素纤维膜。
优选地,所述热塑性聚氨酯溶液为将10wt%~14wt%的热塑性聚氨酯加入到90wt%~86wt%的二甲基亚砜溶剂中,在20~35℃下搅拌至溶解。
优选地,将0.003wt%的氯化锂和0.1wt%的碱木质素加入到配置好的热塑性聚氨酯溶液中,在20~35℃下搅拌至溶解。
优选地,所述步骤S2具体为:首先将制得的聚氨酯纤维膜洗净烘干,然后置于1mmol/L氯化钙溶液中,以3℃/min的升温速率加热至90℃,再加入5mL的1.0g/L杜仲提取物溶液,调节pH至6.25~9.15,反应30min,得到抑菌性能的纤维膜材料。
本发明还提供了一种抑菌纤维膜材料,所述的抑菌纤维膜材料是由上述所述的方法制备得到的。
本发明还提供了一种抑菌纤维膜口罩,所述的口罩的材质为上述的抑菌纤维膜材料。
本发明由于采用以上技术方案,使其与现有技术相比具有以下的优点和积极效果:
本发明将具有抗菌消炎的杜仲提取物与纤维膜结合,成功制得具有抑菌效果的纤维膜,由于杜仲提取物中含有抗菌消炎的绿原酸,采用本发明的方法可以将绿原酸结合到聚氨酯纤维膜上,使聚氨酯纤维膜具有抑菌效果;优选纤维膜材料是聚氨酯/木质素纤维膜,木质素结构上存在的酚类化合物和不同的含氧官能团赋予了其一定的抑菌活性,将其加入纤维膜材料的制备中,可以有效增强材料的抑菌性能。并且木质素是一种存在于植物体内的天然高分子化学物,在提高材料以及性能的同时不会带来环境污染。是一种可降解环保的抑菌口罩材料。
本发明优选实施例将氯化钙与杜仲提取物混合一起应用到纤维膜上,是由于钙与杜仲提取物中的绿原酸可以形成螯合物,并且该螯合物具有优异的抑菌性能,对病菌等有害物质具有有效的吸附作用,同时钙与绿原酸形成了螯合物,抑菌效果更加持久,稳定性更好,抑菌效果更加持久。并且生物法制备钙与杜仲提取物中的绿原酸形成的螯合物,反应条件温和、对环境无污染,可改善常规物理、化学制备方法设备要求高,耗能大、环境污染高等缺点。
具体实施方式
以下结合具体实施例对本发明提出的一种抑菌纤维膜材料及其制备方法及抑菌纤维膜口罩作进一步详细说明。根据下面说明,本发明的优点和特征将更清楚。
实施例1
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL 1mmol/L 氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入 5mL1.0g/L杜仲提取物溶液,调节pH至6.25后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例2
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL 1mmol/L 氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入5mL1.0 g/L杜仲提取物溶液,调节pH至7.26后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例3
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL 1mmol/L 氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入 5mL1.0g/L杜仲提取物溶液,调节pH至8.18后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例4
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL 1mmol/L 氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入 5mL1.0g/L杜仲提取物溶液,调节pH至9.15后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例5
将热塑性聚氨酯(10wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL 1mmol/L 氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入 5mL1.0g/L杜仲提取物溶液,调节pH至8.18后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例6
将热塑性聚氨酯(14wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料。洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL 1mmol/L 氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入5mL 1.0 g/L杜仲提取物溶液,调节pH至8.18后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例7
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL去离子水的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入5mL1.0g/L杜仲提取物溶液,调节pH至9.15后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例8
将热塑性聚氨酯(14wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料。洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL去离子水锥形瓶中,以3℃/min的升温速率加热至90℃,再加入5mL1.0g/L杜仲提取物溶液,调节pH至8.18后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例9
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后,取15cm×15cm的纤维膜置于含有95mL1mmol/L氯化钙溶液的锥形瓶中,以3℃/min的升温速率加热至90℃,再加入5mL 1.0g/L杜仲提取物溶液,调节pH至8.18后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
实施例10
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯纤维膜材料,洗涤烘干后,取 15cm×15cm的纤维膜置于含有95mL 1mmol/L氯化钙溶液的锥形瓶中,以 3℃/min的升温速率加热至90℃,再加入5mL 1.0g/L杜仲提取物溶液,调节 pH至8.18后反应30min,反应完成后取出纤维膜,反复冲洗,室温下干燥。
对比例1:
将热塑性聚氨酯(12wt%)加入二甲基亚砜溶剂(92wt%)中,常温下搅拌至溶解,再将氯化锂(0.003wt%)、碱木质素(0.1wt%)加入已溶解的聚氨酯溶液中,继续搅拌至完全溶解,通过静电纺丝设备制备聚氨酯/木质素纤维膜材料,洗涤烘干后备用。
对比例2:将质量比为3.5∶1的聚氨酯(PU)和二氧化钛(TiO2)共混静电纺丝,制备得TiO2/PU复合纳米纤维,在聚氨酯纤维膜上负载TiO2颗粒。
根据GB 20944.3-2008-T《纺织品抗菌性能的评价第3部分:振荡法》测试以上实施例和对比例的纤维膜材料的抗菌性,结果如下表:
表1不同纤维膜的抑菌性能
从上表的结构可知:实施例1-10与对比例相比,不管是抑制金黄葡萄球菌或大肠杆菌,抑菌性能均好于对比例,但在实施例7和实施例8中,虽然引入了杜仲提取物,但是没有引入钙,使钙与杜仲提取物中的绿原酸反应形成螯合物,使最终得到的纤维素的抑菌性相对于使杜仲提取物中的绿原酸以螯合物形式存在纤维膜中的抑菌性稍微下降一些;在实施例9中制备纤维膜时没有引入氯化锂,但是最终的纤维膜材料的抑菌性能与实施例1-6的抑菌性能相差不大;实施例10中仅引入钙与杜仲提取物中的绿原酸形成的螯合物,而没有引入碱木质素,纤维膜的抑菌性能有所下降,但仍表现出较好的抑菌性能;对比例1中没有引入杜仲提取物,仅引入了碱木质素,抑菌性能有较大下降,呈现出无抑菌性能;而对比例2中是在聚氨酯纤维膜上负载二氧化钛颗粒,抑菌性能效果也相对下降。因此,只有同时将钙与杜仲提取物中的绿原酸形成的螯合物和碱木质素同时引入聚氨酯纤维膜,表现出的抑菌效果更好。
通过对比实施例1-10可知,只有在聚氨酯的溶解浓度为12wt%,反应 pH为8.18时,纤维膜表现出了最佳抑菌性能,高达99.5%以上。
将实施例1-10和对比例1-2的纤维膜放置在湿度为90%,温度37℃条件下,4h后测试纤维膜的抑菌性,与之前的抑菌性对比
表二湿度为90%条件下放置4h后不同纤维膜的抑菌性能
由上表可发现,实施例制备的纤维膜由于钙与杜仲提取物中的绿原酸形成的螯合物是稳定嵌入在纤维膜中的,因此在湿度为90%,温度37℃条件下,放置4h后纤维膜的抑菌性能仍然变化不大;实施例7和8中杜仲提取中的绿原酸没有以螯合物的形式存在纤维膜中,抑菌性能的持久性有所下降;对比例4中是将二氧化钛加入聚氨酯制备抑菌材料,但是在湿度为90%,温度37℃条件下,放置4h后,其抑菌性能也明显下降。
综上,本发明提供的纤维膜材料制备方法以及由该方法制备得到的纤维膜具有较好的抑菌性能,并且抑菌更加持久,将由该纤维膜制备的口罩的抑菌性能更好,抑菌效果更加持久。
上面结合具体实施例对本发明的实施方式作了详细说明,但是本发明并不限于上述实施方式。即使对本发明做出各种变化,倘若这些变化属于本发明权利要求及其等同技术的范围之内,则仍落入在本发明的保护范围之中。
Claims (6)
1.一种抑菌纤维膜材料的制备方法,其特征在于,包括以下步骤:
S1:制备聚氨酯纤维膜:配置热塑性聚氨酯溶液,将氯化锂和碱木质素加入到配置的热塑性聚氨酯溶液中,搅拌、溶解;然后通过静电纺丝设备制备聚氨酯纤维膜;
S2:首先将制得的聚氨酯纤维膜置于氯化钙溶液中,加热后再加入杜仲提取物溶液,调节pH反应后,得到抑菌性能的纤维膜材料。
2.根据权利要求1所述的抑菌纤维膜材料的制备方法,其特征在于,所述热塑性聚氨酯溶液为将10wt%~14wt%的热塑性聚氨酯加入到90wt%~86wt%的二甲基亚砜溶剂中,在20~35℃下搅拌至溶解。
3.根据权利要求2所述的抑菌纤维膜材料的制备方法,其特征在于,将0.003wt%的氯化锂和0.1wt%的碱木质素加入到配置好的热塑性聚氨酯溶液中,在20~35℃下搅拌至溶解。
4.根据权利要求1所述的抑菌纤维膜材料的制备方法,其特征在于,所述步骤S2具体为:首先将制得的聚氨酯纤维膜洗净烘干,然后置于1mmol/L氯化钙溶液中,以3℃/min的升温速率加热至90℃,再加入5mL的1.0g/L杜仲提取物溶液,调节pH至6.25~9.15,反应30min,得到抑菌性能的纤维膜材料。
5.一种抑菌纤维膜材料,其特征在于,所述的抑菌纤维膜材料是由权利要求1-4任意一项所述的方法制备得到的。
6.一种抑菌纤维膜口罩,其特征在于,所述口罩的材质为权利要求5所述的抑菌纤维膜材料。
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